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本文建立双通道离子色谱电导检测器同时测定爆炸残留物中的12种无机离子(NO_2~-,NO_3~-;Cl~-,ClO_3~-,ClO_4~-,SCN~-,SO_4~(2-),S_2O_3~(2-);Na~+,NH_4~+,K~+,Mg~(2+))的方法。样品经水溶、离心、过滤并过0.45μm半渗透膜;阴离子以Metrohm A Supp5 250mm×4mm的阴离子交换柱为分析柱,采用12mmol碳酸钠、1mmol碳酸氢钠、1mmol对氰酚、10%丙酮水溶液作流动相;阳离子以C4 150mm×4mm阳离子交换分离柱,以1.7mmol硝酸、0.7mmol吡啶二羧酸水溶液作流动相。结果表明上述12种离子一次进样就能全部筛选检测,各离子在0~20mg/L之间线性良好,线性相关系数r~2为0.9924~0.9999,检出限在0.01~0.1mg/L之间,加标回收率在86.2%以上。此法快速、准确、简便,能同时筛选常见的12种爆炸残留无机离子,可以跟踪原起爆炸药和爆炸残留物之间的关系,为推断原起爆炸药的种类提供依据。
In this paper, we established a two-channel ion conductivity detector for the simultaneous determination of 12 kinds of inorganic ions (NO 2 -, NO 3 -, Cl ~ -, ClO 3 ~ -, ClO 4 ~ -, SCN ~ -, SO 4 2- ), S_2O_3 ~ (2 -); Na ~ +, NH_4 ~ +, K ~ +, Mg ~ (2+)). The sample was water-soluble, centrifuged, filtered and passed through a 0.45 μm semi-permeable membrane. Anions were analyzed on an anion exchange column of Metrohm A Supp5 250 mm × 4 mm using 12 mmol sodium carbonate, 1 mmol sodium bicarbonate, 1 mmol p-cyanohydrin, 10% As mobile phase; cation to C4 150mm × 4mm cation exchange column, with 1.7mmol nitric acid, 0.7mmol dipicolinic acid aqueous solution as the mobile phase. The results showed that the above 12 kinds of ions could be selected and tested by single injection. The linearity of each ion was between 0 ~ 20mg / L, the linear correlation coefficient r ~ 2 was 0.9924 ~ 0.9999, the detection limit was 0.01 ~ 0.1mg / L Between the spiked recoveries above 86.2%. This method is fast, accurate and simple. It can screen 12 common types of residual inorganic ions at the same time. It can track the relationship between the original explosive and the explosive residue, and provide the basis for inferring the type of original explosive.